A four-layer co-extruded infusion film and a preparation process thereof

Abstract

The present application relates to a kind of four-layer co-extrusion infusion film and its preparation process, using four-layer structure, film is composed of A layer, B layer, C layer and D layer. Wherein, A layer is the outer layer of product, thickness is 15-25 μm, is composed of polypropylene and styrene-ethylene-butadiene hydrogen block copolymer. B layer is the secondary outer layer of product, thickness is 10-15 μm, is composed of modified linear low density polyethylene. C layer is the intermediate layer of product, thickness is 130-160 μm, is composed of modified polyethylene. D layer is the inner layer of product, thickness is 10-30 μm, is composed of ethylene-propylene copolymer and styrene-ethylene-butadiene hydrogen block copolymer. The present application adopts four-layer co-extrusion down blowing process, and prepares the packaging suitable for various infusion. The present application not only guarantees the light transmittance, low temperature heat sealing property, heat sealing strength, printability, resistance to 121 ℃ cooking and other properties of film. Film material is compatible with the softness of traditional five-layer co-extrusion infusion film and the high strength characteristics of three-layer co-extrusion infusion film.

Description

TECHNICAL FIELD

[0001] The present application relates to a kind of intravenous infusion medicine packaging film, and specifically relates to a kind of four-layer co-extrusion infusion film and its preparation process. BACKGROUND

[0002] The infusion package widely used at present is glass bottle and hard plastic bottle, which has a weak point, i.e. an air circuit needs to be formed during use, thereby increasing secondary pollution in the infusion process, especially in places where bacteria are more and the sanitary conditions are poor.

[0003] The non-PVC multi-layer co-extrusion film has the following characteristics: (1) compatibility, the material used in the non-PVC multi-layer co-extrusion film is inert material, which has good drug compatibility, and avoids the precipitation of small molecule additives to cause drug pollution; (2) safety, the non-PVC multi-layer co-extrusion film material has excellent flexibility, which can avoid air permeation; the non-PVC multi-layer co-extrusion film material has excellent light transmission, which is beneficial to check visible foreign matters in the drug; the non-PVC multi-layer co-extrusion film material has excellent low-temperature resistance, which can meet the low-temperature transportation and is not easy to break; the non-PVC multi-layer co-extrusion film material has excellent sterilization adaptability, which can meet the high-temperature sterilization at 121 ℃. The above performances build the safety of the entire drug use. (3) environmental protection, the non-PVC multi-layer co-extrusion film material is mostly degradable material, which has no pollution to the environment.

[0004] At present, the non-PVC multi-layer co-extrusion infusion film commonly seen on the market includes three-layer co-extrusion infusion film and five-layer co-extrusion infusion film. The three-layer co-extrusion infusion film has low cost and high strength, but has poor flexibility and is easy to become brittle, especially under low-temperature conditions, which can easily cause liquid leakage. The five-layer co-extrusion infusion film has good flexibility and good barrier property, which can meet the use under various conditions, but the outer polyester material has high requirements for equipment and high cost.

[0005] Therefore, the present application proposes a four-layer film which has the advantages of both five-layer co-extrusion infusion film and three-layer co-extrusion infusion film, and meets the performance requirements of intravenous infusion packaging materials. SUMMARY

[0006] The present application provides a four-layer co-extrusion infusion film and its preparation process to solve the above problems. The film has the advantages of non-toxicity, good printability, high light transmission, high heat sealing strength, good flexibility, etc.

[0007] The four-layer co-extrusion infusion film according to the present application is a four-layer composite film, and the composition from the outer layer to the inner layer is: polypropylene / styrene-ethylene-butadiene hydrogen block copolymer, modified polyethylene / ethylene-propylene copolymer, modified polyethylene, ethylene-propylene copolymer / styrene-ethylene-butadiene hydrogen block copolymer.

[0008] The outer layer A is composed of the following raw materials in the following mass percentages: 85%–95% polypropylene, 5%–15% styrene-ethylene-butadiene hydrogenated block copolymer, and has a thickness of 15–25 μm;

[0009] The outermost layer B is composed of the following raw materials by mass percentage: 75%–85% modified polyethylene, 15%–25% ethylene-propylene copolymer, with a thickness of 5–15 μm;

[0010] The intermediate layer C is composed of the following raw materials by mass percentage: 100% modified polyethylene with a thickness of 130–170 μm;

[0011] The inner layer D is composed of the following raw materials in the following mass percentages: 80% to 90% ethylene-propylene copolymer, 10% to 20% styrene-ethylene-butadiene hydrogenated block copolymer, with a thickness of 10 to 30 μm.

[0012] The polypropylene used in the outer layer of the four-layer co-extruded infusion membrane has a melting point between 145 and 160°C and a density of 0.87 to 0.92 g / cm³. 3 The melt flow index is 4.0–8.0 g / 10 min. It is a hydrogenated block copolymer of styrene-ethylene-butadiene with a density of 0.87–0.92 g / cm³. 3 The melt flow index is 2.0–6.0 g / 10 min. The main function of the outer layer is to provide the bag with weather resistance, barrier properties, and heat resistance during high-temperature sterilization and heat sealing.

[0013] The modified polyethylene used in the outermost layer of the four-layer co-extruded infusion membrane has a melting point between 80 and 110°C, a density of 0.9 to 0.92 g / cm³, and a melt index of 0.5 to 3.0 g / 10 min. The ethylene-propylene copolymer has a melting point between 100 and 130°C, a density of 0.89 to 0.92 g / cm³, and a melt index of 1.0 to 7.0 g / 10 min. This layer primarily serves to bond the intermediate and outer layers.

[0014] The modified polyethylene used in the intermediate layer of the four-layer co-extruded infusion membrane has a melting point between 80 and 130°C and a density of 0.90 to 0.92 g / cm³. 3 The melt flow index is 0.5–3.0 g / 10 min. The main functions of this layer are barrier properties, flexibility, good transparency, and good low-temperature performance.

[0015] The ethylene-propylene copolymer used in the inner layer of the four-layer co-extruded infusion membrane has a melting point between 120 and 145°C and a density of 0.85 to 0.93 g / cm³. 3, a melt index of 1.0-7.0 g / 10 min. Styrene-ethylene-butadiene hydrogenated block copolymer, density of 0.87-0.92 g / cm 3 , a melt index of 2.0-6.0 g / 10 min. The main role of this layer is to improve good drug compatibility, low absorption, low adsorption and wide heat sealing temperature range.

[0016] The total thickness of the four-layer co-extrusion film is 170-250 μm.

[0017] The application also provides a preparation process of the above four-layer co-extrusion film, comprising the following steps:

[0018] Step 1, the raw materials of each layer are respectively drawn into the material bin of each extruder, the material bin feeding screw feeds the plastic particles to the mixing hopper by pre-setting the mass percentage, and then the plastic particles are melted and plasticized by controlling the heating temperature of each section of the extruder, and the melted mixture is obtained;

[0019] Step 2, the completely plasticized mixture is filtered through a filter screen to remove impurities, and is respectively extruded through the connecting pipeline and the die, and the rotating speed of the extruder is controlled, so that the four layers are combined together at the die, and the four-layer co-extrusion film is formed.

[0020] Further, in step 1, the heating temperature of the outer layer extruder 9 zone is respectively: 30-70℃, 160-200℃, 180-220℃, 200-230℃, 200-235℃, 200-235℃, 200-240℃, 200-240℃, 200-240℃.

[0021] Further, in step 1, the heating temperature of the outer layer extruder 9 zone is respectively: 30-70℃, 160-200℃, 180-220℃, 200-230℃, 200-235℃, 200-235℃, 200-240℃, 200-240℃, 200-240℃.

[0022] Further, in step 1, the heating temperature of the outer layer extruder 9 zone is respectively: 30-70℃, 160-200℃, 180-220℃, 200-230℃, 200-235℃, 200-235℃, 200-240℃, 200-240℃, 200-240℃.

[0023] Further, in step 1, the heating temperature of the outer layer extruder 9 zone is respectively: 30-70℃, 160-200℃, 180-220℃, 200-230℃, 200-235℃, 200-235℃, 200-240℃, 200-240℃, 200-240℃.

[0024] Further, the respective control of the rotating speed of the extruder in step 2 is specifically: the outer layer extruder: 20-50 rpm, the secondary outer layer extruder: 30-50 rpm, the intermediate layer extruder: 40-80 rpm, and the inner layer extruder: 20-50 rpm.

[0025] Further, the raw materials are re-distributed and extruded through a die after being extruded through the screw of the extruder in step 2, and the temperature of the die is 180-240℃. A plane superposition die is used, and the film bubble is formed by the clean air after being extruded through the die, the blowing ratio is between 1.5-3, the blowing pressure is 0.4-0.8 MPa, the cooling water temperature is 15-30℃, and the flow rate is 1000-3000 L / h. The film bubble is cooled by the clean air and purified water, and is folded and flattened by a herringbone clamp before being wound by a winding machine.

[0026] Compared with the existing multi-layer co-extrusion film for infusion, the beneficial effects of the present application are:

[0027] (1) The four-layer structure adopted by the present application has better flexibility than the three-layer co-extrusion film for infusion, and even in an environment below 0℃, the film still has good softness, puncture resistance and impact performance.

[0028] (2) The four-layer structure adopted by the present application has better mechanical strength and lower cost than the traditional five-layer co-extrusion film for infusion, and the outer layer material is replaced by polypropylene instead of ester copolymer, which is not easily affected by the raw material manufacturers. DETAILED DESCRIPTION

[0029] The four-layer co-extrusion film of the present application is composed of an outer layer, a secondary outer layer, an intermediate layer and an inner layer.

[0030] The total thickness of the four-layer co-extrusion film is 170-250 μm.

[0031] The outer layer is composed of the following raw materials in mass percentage: polypropylene 90%, styrene-ethylene-butadiene hydrogenated block copolymer 10%; wherein the melt flow rate of the polypropylene measured according to GB-T3682 at 230℃ / 2.16 Kg is 7.0 g / 10 min; the melt flow rate of the styrene-ethylene-butadiene hydrogenated block copolymer measured according to GB-T3682 at 230℃ / 2.16 Kg is 3.0 g / 10 min; and the thickness is 15-25 μm.

[0032] The preparation of the secondary outer layer is composed of the following raw materials in mass percentage: modified polyethylene 85%, ethylene propylene copolymer 15%; wherein the modified polyethylene has a melt flow rate of 1.0 g / 10 min at 190℃ / 2.16 Kg measured according to GB-T3682; the ethylene propylene copolymer has a melt flow rate of 5.5 g / 10 min at 190℃ / 2.16 Kg measured according to GB-T3682; the thickness is 5-15 μm;

[0033] The preparation of the intermediate layer is composed of the following raw materials in mass percentage: modified polyethylene 100%, wherein the modified polyethylene has a melt flow rate of 1.0 g / 10 min at 190℃ / 2.16 Kg measured according to GB-T3682, the thickness is 130-170 μm;

[0034] The preparation of the inner layer is composed of the following raw materials in mass percentage: ethylene-propylene copolymer 80%, styrene-ethylene-butadiene hydrogenated block copolymer 20%; wherein the ethylene-propylene copolymer has a melt flow rate of 7.0 g / 10 min at 230℃ / 2.16 Kg measured according to GB-T3682; the styrene-ethylene-butadiene hydrogenated block copolymer has a melt flow rate of 3.0 g / 10 min at 230℃ / 2.16 Kg measured according to GB-T3682; the thickness is 10-30 μm.

[0035] The preparation process of the four-layer co-extrusion infusion film comprises the following steps:

[0036] Step 1, the raw materials of the layers are respectively drawn into the material bins of the extruders, the material feeding screw pre-sets the mass percentage feeding, the plastic particles are transported to the mixing hopper, after mixing, they are fed into the heating sections of the extruders, the plastic particles are melted and plasticized by controlling the heating temperature of each section of the extruder, and the melted mixtures are respectively obtained;

[0037] Step 2, the completely plasticized melted mixtures are filtered through the filter screen to remove impurities, and are respectively extruded through the connecting pipelines and the die, the rotating speeds of the extruders are respectively controlled, the four layers are combined together at the die, and the four-layer co-extrusion film is formed.

[0038] In step 1, the heating temperatures of the outer layer extruder 9 are respectively 50-60℃, 160-170℃, 190-200℃, 210-220℃, 220-235℃, 220-235℃, 220-235℃, 220-235℃, and 220-235℃;

[0039] The heating temperatures of the secondary outer layer extruder 9 are respectively 50-60℃, 100-110℃, 150-160℃, 200-210℃, 220-235℃, 220-235℃, 220-235℃, 220-235℃, and 220-235℃;

[0040] The heating temperature of the intermediate layer extruder 8 is respectively 50-60℃, 110-120℃, 140-150℃, 180-210℃, 220-230℃, 220-230℃, 220-230℃, 220-230℃.

[0041] The heating temperature of the inner layer extruder 9 is respectively 30-40℃, 190-200℃, 190-200℃, 190-200℃, 190-200℃, 220-230℃, 220-230℃, 220-230℃, 220-230℃.

[0042] The specific control of the extruder speed in step 2 is as follows: the outer layer extruder is 20-50 revolutions per minute, the secondary outer layer extruder is 30-50 revolutions per minute, the intermediate layer extruder is 40-80 revolutions per minute, and the inner layer extruder is 20-50 revolutions per minute.

[0043] After the raw materials are extruded by the extruder screw, they are re-distributed and extruded by the die head, the die head temperature is 200-240℃; a plane superposition die head is used, after extrusion by the die head, a film bubble is formed by the clean air blowing down, the blowing ratio is between 1.5-2, the blowing pressure is 0.4MPa-0.8MPa, the cooling water temperature is 15℃-30℃, and the flow rate is 0000L / h-3000L / h; the film bubble is cooled by the clean air and purified water, after folding and flattening, it is wound into a winding machine for winding.

[0044] The specific implementation is shown in Table 1.

[0045] Table 1

[0046] Outer layer (pm) Sub-outer layer (pm) Intermediate layer (pm) Inner layer (pm) Example 1 20 10 145 25 Example 2 25 10 160 25 Example 3 15 10 130 15

[0047] According to the national standard YBB00112005-2015, the performance of the film is tested, and the relevant performance is as follows:

[0048]

[0049]

[0050] The above only describes the preferred embodiments of the present application and is not intended to limit the present application. Any modification, equivalent replacement and improvement made by those skilled in the art within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A preparation process for a four-layer co-extruded infusion membrane, characterized in that, Includes the following steps: Step 1: The raw materials of each layer are fed into the extruder hoppers respectively. The feed screw of the hopper feeds the plastic particles by a preset mass percentage and delivers them to the mixing hopper. After mixing, the particles enter the heating sections of the extruder. The plastic particles are melted and plasticized by controlling the heating temperature of each section of the extruder to obtain molten mixtures. Step 2: The fully plasticized molten mixture is filtered through a filter screen to remove impurities, and then extruded through a connecting pipe and a die head. The speed of the extruder is controlled separately, and the four layers are laminated together at the die to form a four-layer co-extruded film. In step 1, the heating temperatures of the nine zones of the outer extruder are 50~60℃, 160~170℃, 190~200℃, 210~220℃, 220~235℃, 220~235℃, 235~240℃, 235~240℃, and the outer layer thickness is 25μm. The heating temperatures of the nine zones of the secondary outer layer extruder are 50~60℃, 100~110℃, 150~160℃, 200~210℃, 220~235℃, 220~235℃, 220~235℃, 220~235℃, and the thickness of the secondary outer layer is 10μm. The heating temperatures of the eight zones of the intermediate layer extruder are 50~60℃, 110~120℃, 140~150℃, 180~210℃, 220~230℃, 220~230℃, 220~230℃, 220~230℃, and the thickness of the intermediate layer is 160μm. The heating temperatures of the nine zones of the inner layer extruder are 30~40℃, 190~200℃, 190~200℃, 190~200℃, 190~200℃, 220~230℃, 220~230℃, 220~230℃, and the inner layer thickness is 25μm. The specific speed control of the extruders mentioned in step 2 is as follows: outer layer extruder: 20~50 rpm, second outer layer extruder: 30~50 rpm, middle layer extruder: 40~80 rpm, inner layer extruder: 20~50 rpm; The raw material is extruded by the screw of the extruder and then redistributed through the die head. The die head temperature is 200~240℃. A planar superimposed die head is used. After extrusion through the die head, clean air forms a downblown film bubble with a blow-up ratio between 1.5 and 2, a blowing pressure of 0.4MPa~0.8MPa, a cooling water temperature of 15℃~30℃, and a flow rate of 3000L / h. The film bubble is cooled by clean air and purified water, folded flat, and then enters the winding machine for winding. The outer layer is composed of the following raw materials in the indicated mass percentages: 90% polypropylene and 10% styrene-ethylene-butadiene hydrogenated block copolymer; wherein the melt flow rate of the polypropylene at 230℃ / 2.16Kg, as measured according to GB-T3682, is 7.0 g / 10 min; and the melt flow rate of the styrene-ethylene-butadiene hydrogenated block copolymer at 230℃ / 2.16Kg, as measured according to GB-T3682, is 3.0 g / 10 min. The outermost layer is prepared from the following raw materials in the indicated mass percentages: 85% modified polyethylene and 15% ethylene-propylene copolymer; wherein the melt flow rate of the modified polyethylene at 190℃ / 2.16Kg, as measured according to GB-T3682, is 1.0 g / 10 min; and the melt flow rate of the ethylene-propylene copolymer at 190℃ / 2.16Kg, as measured according to GB-T3682, is 5.5 g / 10 min. The intermediate layer is composed of the following raw materials by mass percentage: 100% modified polyethylene, wherein the melt flow rate of the modified polyethylene at 190℃ / 2.16Kg is 1.0g / 10min as measured according to GBT3682; The inner layer is composed of the following raw materials in the indicated mass percentages: 80% ethylene-propylene copolymer and 20% styrene-ethylene-butadiene hydrogenated block copolymer; wherein the melt flow rate of the ethylene-propylene copolymer at 230℃ / 2.16Kg, as measured according to GB-T3682, is 7.0 g / 10 min; and the melt flow rate of the styrene-ethylene-butadiene hydrogenated block copolymer at 230℃ / 2.16Kg, as measured according to GB-T3682, is 3.0 g / 10 min.

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